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JP3591010B2 - Method for producing toner for developing electrostatic images - Google Patents
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JP3591010B2 - Method for producing toner for developing electrostatic images - Google Patents

Method for producing toner for developing electrostatic images Download PDF

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Publication number
JP3591010B2
JP3591010B2 JP26913194A JP26913194A JP3591010B2 JP 3591010 B2 JP3591010 B2 JP 3591010B2 JP 26913194 A JP26913194 A JP 26913194A JP 26913194 A JP26913194 A JP 26913194A JP 3591010 B2 JP3591010 B2 JP 3591010B2
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Japan
Prior art keywords
toner
kneading
fine powder
resin
screw
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
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JP26913194A
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Japanese (ja)
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JPH0895296A (en
Inventor
幹夫 海野
隆 新卓
隆次 竹原
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Mitsubishi Chemical Corp
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Mitsubishi Chemical Corp
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Priority to JP26913194A priority Critical patent/JP3591010B2/en
Publication of JPH0895296A publication Critical patent/JPH0895296A/en
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G9/00—Developers
    • G03G9/08—Developers with toner particles
    • G03G9/0802—Preparation methods
    • G03G9/081—Preparation methods by mixing the toner components in a liquefied state; melt kneading; reactive mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B29B7/482—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws provided with screw parts in addition to other mixing parts, e.g. paddles, gears, discs
    • B29B7/483—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws provided with screw parts in addition to other mixing parts, e.g. paddles, gears, discs the other mixing parts being discs perpendicular to the screw axis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B29B7/488—Parts, e.g. casings, sealings; Accessories, e.g. flow controlling or throttling devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58—Component parts, details or accessories; Auxiliary operations
    • B29B7/60—Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material
    • B29B7/603—Component parts, details or accessories; Auxiliary operations for feeding, e.g. end guides for the incoming material in measured doses, e.g. proportioning of several materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58—Component parts, details or accessories; Auxiliary operations
    • B29B7/72—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/84—Venting or degassing ; Removing liquids, e.g. by evaporating components
    • B29B7/845—Venting, degassing or removing evaporated components in devices with rotary stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/86—Component parts, details or accessories; Auxiliary operations for working at sub- or superatmospheric pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/285—Feeding the extrusion material to the extruder
    • B29C48/297—Feeding the extrusion material to the extruder at several locations, e.g. using several hoppers or using a separate additive feeding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
    • B29C48/39—Plasticisers, homogenisers or feeders comprising two or more stages a first extruder feeding the melt into an intermediate location of a second extruder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B29C48/405—Intermeshing co-rotating screws
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50—Details of extruders
    • B29C48/505—Screws
    • B29C48/57—Screws provided with kneading disc-like elements, e.g. with oval-shaped elements

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Developing Agents For Electrophotography (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Description

【０００１】
【産業上の利用分野】
本発明は電子写真法、静電記録等において使用される静電荷像現像用トナーの製造方法に関するものである。
【０００２】
【従来の技術】
電子複写機等で使用される現像剤は、その現像工程において、例えば静電荷像が形成されている感光体等の像担持体に一旦付着され、次に転写工程において感光体から転写紙に転写された後、定着工程においてコピー紙面に定着される。その際、潜像保持面上に形成される静電荷像を現像するための現像剤として、キャリアとトナーから成る二成分現像剤及びキャリアを必要としない一成分現像剤（磁性トナー、非磁性トナー）が知られている。
該現像剤に含有されるトナーとしては、正荷電性トナーと負荷電性トナーがあり、従来より正荷電性トナーに帯電性を付与するものとしては、ニグロシン系染料、第４級アンモニウム塩等、また負荷電性トナーに帯電性を付与するものとしては含金染料等の帯電制御剤やキャリアに所定の帯電性を付与するコーティング剤等が知られていた。
【０００３】
通常行われるトナー製造フローの一例を図１に示す。まず樹脂と着色剤等の材料を所定量配合、混合し、ニーダーで溶融混練し、冷却後粉砕し、分級する。更に、分級トナーと外添剤を攪拌、混合した後、粗大物を篩別し、容器に充填する。
従来、発生したトナー微粉については、特開平５−３４９７６号公報などに記載されている様に、環境面及び生産コスト面などを考慮して原料配合・混合工程へ所定量リサイクルして再利用されていた。しかしながら、従来のトナー微粉リサイクル方法では、トナー微粉が混練機で再度溶融混練される際に、トナー微粉中の樹脂の分子切断が再度起こり、樹脂の分子量低下によるトナーホットオフセットなどの定着性能の悪化、機械的強度の低下による耐久性能の悪化などを引き起こし好ましくなかった。特に、トナー中の樹脂の分子量低下は架橋成分を含んだ樹脂、または少なくとも低分子量体と高分子量体から成る分子量ピークを２つ以上有する樹脂等を使用した場合に顕著に起こりやすい傾向にある。また、トナー微粉が原料に混ざると、微粉を含まない原料に比し、（ａ）原料の均一混合がしにくく、トナー組成が不均一になること、（ｂ）原料の嵩密度が小さくなり連続的に混練機に原料を供給した時の食い込みが悪化し、トナー生産性が低下し、練り時のシェアがかかりずらくなり添加物の分散性が不良になること、（ｃ）原料混合した後の貯蔵・供給容器から連続的に混練機に供給する時に貯蔵・供給容器内部で原料と微粉の粒度・比重差により、生産過程の途中でトナー組成が不均一になることなどから、ひいてはトナー性能の悪化を招きやすくなり、好ましくなかった。
【０００４】
特に、近年では（ａ）複写機等の高速度化、ファーストコピー時間短縮化などに伴いトナーに使用されるバインダー樹脂のフロー軟化温度は定着面より低い温度に設計されるため、機械的強度が低下し過粉砕され易く、必要以上に微粉が発生すること、（ｂ）複写物の高画質化などに伴いトナーを小粒径化すると、分級効率が低下し、微粉が従来以上に増加すること等により、トナー微粉リサイクル量が増加し、トナー性能の劣化なしに生産性を確保することが難しくなってきた。
【０００５】
【発明が解決しようとする課題】
従って、本発明の第１の目的はトナーの分子量変化の少ない、定着性能、耐久性能の優れたトナーの製造方法を提供することにある。第２の目的はトナー中の添加物の分散性がよく、均一な組成のトナーの製造方法を提供することにある。第３の目的は環境依存性が少なく、貯蔵安定性に優れたトナーを提供することにある。第４の目的は連続コピーした場合でも、画像特性、画像品質、帯電特性等が安定していて、耐久性能に優れたトナーを提供することにある。第５の目的は微粉リサイクルしても生産性のよいトナー製造方法を提供することにある。
【０００６】
【課題を解決するための手段】
本発明者らが種々鋭意検討した結果、トナー微粉を混練工程の途中にリサイクルして再利用することでトナー性能が改善できることを見い出して、本発明に到達した。すなわち、本発明の要旨は、少なくとも樹脂及び着色剤を配合、混合した後、混練し、次いで粉砕、分級するとともに、発生したトナー微粉を混練工程に戻して再利用してトナーを得る静電荷像現像用トナーの製造方法において、混練工程で使用される装置がニーディング部スクリュからなるニーディングゾーンを少なくとも２つ有する連続式押出機であり、トナー微粉を該連続式押出機の主原料供給口からダイの方向に位置
する第１のニーディングゾーンと第２のニーディングゾーンとの間に供給することを特徴とする静電荷像現像用トナーの製造方法に存する。
【０００７】
【作用】
以下、本発明を詳細に説明する。
本発明で用いる樹脂としてはトナーに適した公知の種類のものが使用できる。例えば、ポリスチレン、ポリクロロスチレン、ポリ−α−メチルスチレン、スチレン−クロロスチレン共重合体、スチレン−プロピレン共重合体、スチレン−ブタジエン共重合体、スチレン−塩化ビニル共重合体、スチレン−酢酸ビニル共重合体、スチレン−アクリル酸エチル共重合体（スチレン−アクリル酸メチル共重合体、スチレン−アクリル酸エチル共重合体、スチレン−アクリル酸ブチル共重合体、スチレン−アクリル酸オクチル共重合体及びスチレン−アクリル酸フェニル共重合体等）、スチレン−メタクリル酸エステル共重合体（スチレン−メタクリル酸メチル共重合体、スチレン−メタクリル酸エチル共重合体、スチレン−メタクリル酸ブチル共重合体及びスチレン−メタクリル酸フェニル共重合体等）、スチレン−α−クロルアクリル酸メチル共重合体及びスチレン−アクリロニトリル−アクリル酸エステル共重合体等のスチレン系樹脂（スチレンまたはスチレン置換体を含む単重合体または共重合体）、塩化ビニル樹脂、ロジン変性マレイン酸樹脂、フェノール樹脂、エポキシ樹脂、ポリエステル樹脂、ポリエチレン樹脂、ポリプロピレン樹脂、アイオノマー樹脂、ポリウレタン樹脂、シリコーン樹脂、ケトン樹脂、エチレン−エチルアクリレート共重合樹脂、キシレン樹脂、ポリビニルブチラール樹脂、並びにポリカーボネート樹脂等があるが、本発明に用いるのに特に好ましい樹脂としてはスチレン系樹脂、飽和または不飽和ポリエステル樹脂及びエポキシ樹脂等が挙げることができる。また、上記樹脂は単独に使用するに限らず、２種以上併用することもできる。
【０００８】
樹脂のフロー軟化温度（Ｔｍ）としては８０〜１５０℃がよく、更には９０〜１４０℃が好ましい。８０℃未満では紙への定着温度は低くて良好であるが、ホットオフセットが発生しやすく、またトナーが現像槽内部で破砕されやすくなりキャリア表面、ドクターブレードにトナーが固着するスペント現象が発生し、帯電特性の悪化を引き起こし、ひいては現像剤の耐久性能の悪化を招き問題がある。また、１５０℃より高いと紙への定着温度が高い、トナー粉砕性が悪い等の問題がある。
【０００９】
樹脂のガラス転移温度は４５℃以上が好ましく、４５℃未満では４０℃の高温で長時間トナーを放置した場合にトナーの固い凝集或いは固着を招くなど保存安定性が悪く、また、外添工程でトナー凝集物を生成し易い、更に篩別装置のスクリーン、側壁等に付着し凝集物を生成し易いなどの使用上問題がある。
【００１０】
また、樹脂の製造は公知の溶液重合、懸濁重合、塊状重合、乳化重合等により行えばよく、必要に応じ各樹脂成分（例えば、低分子量体、高分子量体等）の重合方法は違えてもよい。更に、トナー臭気面より樹脂中の残存モノマー及び残存溶剤量等の軽沸物成分の総量は２，０００ｐｐｍ以下、中でも特に１，０００ｐｍ以下が好ましい。
本明細書で使用する樹脂の各試験方法を以下に説明する。
【００１１】
〔フロー軟化温度（Ｔｍ）〕
フローテスター（（株）島津製作所社製ＣＦＴ−５００）において、試料１ｇをノズル１ｍｍ×１０ｍｍのダイ、荷重３０ｋｇ、予熱時間５０℃で５分、昇温速度３℃／分の条件下で測定を行い、フロー開始から終了までの距離の中間点の温度を軟化温度とする。
【００１２】
〔ガラス転移温度（Ｔｇ）〕
示差熱分析計（（株）島津製作所社製ＤＴＡ−４０）において、昇温速度１０℃／分の条件で測定した曲線の転移（変曲）開始部に接線を引き、その交点温度をガラス転移温度とする。
本発明で用いる着色剤としては、公知の顔料、染料を用いればよい。例えば、カーボンブラック、酸化チタン、亜鉛華、アルミナホワイト、炭酸カルシウム、群青、紺青、フタロシアニンブルー、フタロシアニングリーン、ハンザイエローＧ、ローダミン系染料、クロムイエロー、キナクリドン、ベンジンイエロー、ローズベンガル、トリアリルメタン系染料、アントラキノン系染料、モノアゾ及びジアゾ系染顔料などの着色剤を単独または２種以上混合して使用できる。着色剤の含有量は、現像により可視像を形成することができるようトナーを着色するに十分な量あればよく、例えば樹脂１００重量部に対して１〜２０重量部、好ましくは３〜１５重量部含有させる。
【００１３】
更に、公知の正荷電性または負荷電性の帯電制御剤を単独または併用してトナーに使用してもよく、その使用量は所望する帯電量見合いで選定すればよく、例えば樹脂１００重量部に対して０．０５〜１０重量部程度が好ましい。正荷電性帯電制御剤としては、例えばニグロシン系染料、第４級アンモニウム塩系化合物、トリフェニルメタン系化合物、イミダゾール系化合物、ポリアミン樹脂などがある。負荷電性帯電制御剤としては、Ｃｒ，Ｃｏ，Ａｌ，Ｆｅ等の金属含有アゾ系染料、サリチル酸金属化合物、アルキルサリチル酸金属化合物、カーリックスアレーン化合物などがある。
【００１４】
更に、必要に応じてその他の内添剤を助剤として単独または併用して使用してもよく、例えば公知の離型剤の低分子量オレフィン重合体、フィラー等が挙げることができる。
まず、本発明のトナー製造フローについて図２に従い一例を説明するが、その要旨を超えない限り以下の説明に何等制限されるものではない。
トナー内添剤として、少なくとも樹脂、着色剤を所定量秤量して配合し、混合する。混合装置の一例としては、ダブルコーン・ミキサー、Ｖ型ミキサー、ドラム型ミキサー、スーパーミキサー、ヘンシェルミキサー、ナウターミキサー等がある。
【００１５】
次に、混練工程では、バッチ式（例えば、加圧ニーダー、バンバリィミキサー等）または連続式の練り機を用いるが、連続生産できる等の優位性から、近年は１軸または２軸押出機が主流であり、例えば、神戸製鋼所社製ＫＴＫ型２軸押出機、東芝機械社製ＴＥＭ型２軸押出機、ケイ・シー・ケイ社製２軸押出機、池貝鉄工社製ＰＣＭ型２軸押出機、栗山製作所社製２軸押出機、ブス社製コ・ニーダー等がよい。
練り後、トナーは２本ロール等で圧延され、空冷・水冷等で冷却する冷却工程を経る。
次いで、粉砕工程では、クラッシャー、ハンマーミル、フェザーミル等で粗粉砕し、ジェットミル、高速ローター回転式ミル等で細粉砕し、段階的に所定トナー粒度まで粉砕する。
【００１６】
粉砕後、慣性分級方式のエルボージェット、遠心力分級方式のミクロプレックス、ＤＳセパレータ等でトナーを分級し、平均粒子径３〜１５μｍのトナーを得る。分級工程で発生したトナー粗粉は粉砕工程に戻して再利用してもよい。
更に、トナーに外添処理する場合には、分級トナーと公知の各種外添剤を所定量配合して、ヘンシェルミキサー、スーパーミキサー等の粉体にせん断力を与える高速攪拌機などで攪拌・混合するのがよい。この際、外添機内部で発熱があり、凝集物を生成し易くなるので、外添機の容器部周囲を水で冷却するなどの手段で温度調整をする方が好ましく、更には外添機容器内部の材料温度は樹脂のガラス転移温度より約１０℃低めの管理温度以下が好適である。
【００１７】
外添剤としては公知の無機または有機の各種外添剤を使用することができるが、特にトナーの流動性向上、凝集性抑制を図る為にチタニア、シリカ、アルミナ、酸化亜鉛、酸化マグネシウム等の無機微粉末が好適である。
外添剤の混合量は、使用する外添剤及びトナー粒子の平均粒径、粒度分布などにより異なるが、所望するトナー流動性を得る量がよく、例えばトナー粒子１００重量部に対して０．０５〜１０重量部、更には０．１〜８重量部が好適である。混合量が０．０５重量部未満では流動性改善効果がなく、高温での貯蔵安定性能が悪く、また混合量が１０重量部より多いと一部遊離した外添剤により感光体にフイルミングを発生したり、現像槽内部に堆積し現像剤の帯電機能の劣化等の障害を引き起こし好ましくない。
【００１８】
また、外添剤は高湿環境下での安定性面より、無機微粉末の場合には公知のシランカップリングなどの処理剤で疎水化処理されたものがより好ましく、更に、帯電性を考慮する場合には負荷電性を付与する処理剤としてはジメチルジクロルシラン、モノオクチルトリクロルシラン、ヘキサメチルジシラザン、シリコーンオイルなど、正荷電性を付与する処理剤としてアミノシランなどを使用すればよい。
この他、トナー外添剤として抵抗調整、研磨剤などの目的で、流動性改善用以外の公知のマグネタイト、ファライト、導電性チタン、酸化アンチモン、酸化錫、酸化セリウム、ハイドロタルサイト類化合物、アクリルビーズ、シリコーンビーズ、ポリエチレンビーズなどの微粉末を適宜混合してもよく、その混合量はトナー１００重量部に対して０．００５〜１０重量部が好ましい。
【００１９】
得られたトナーは、キャリアを使用しない１成分系現像剤（マグネタイト等の磁性物を含有した磁性１成分トナー、または磁性物を含有しない非磁性１成分トナー）、或いは、鉄粉、フェライト、マグネタイト、磁性樹脂キャリア等の磁性キャリアと混合した２成分系現像剤として用いることができる。
本発明のトナー製造方法の一例を図２に示すが、本発明はトナー微粉を混練工程の途中に供給することに特徴があり、特に連続式押出機の途中にトナー微粉を供給する場合に有効に作用する。
【００２０】
図３に連続式押出機の一例を示す。
バレルは５〜１４の１０分割で、その内バレル６〜１４の９バレルとダイ１５は内部又は外部に電気ヒーターを有し、温度制御盤によって温調されるものである。そして、バレル５には上部に主原料供給口１を有し、バレル９、バレル１１、バレル１３の上部にはベント口２、３、４をそれぞれ有する。押出機内部には２条タイプの２つの軸がかみ合わさって同方向に１００〜５００ｒｐｍ程度の高速に回転するスクリュが設けられている。スクリュの構成は適宜選択することができ、例えば図３の様に送り部スクリュ３０とニーディング部スクリュ３１などで構成させればよい。トナー主原料は、主原料ホッパー２０からスクリュフィーダー２１により主原料供給口１に投入され、送り部スクリュー３０に供給される。主原料は徐々に予熱されて行き、第１のニーディング部スクリュ３１で強いシェアがかかることで主原料自体の自己発熱により原料は分散し、固体から溶融状態に変化する。バレル９を通過する時点では主原料は充分に溶融状態になっており、ここでトナー微粉がホッパー２２からスクリュフィーダー２３でベント口２に投入され、トナー微粉と溶融した主原料が一緒になり、その後の送り部スクリュとニーディング部スクリュでトナー微粉が主原料に混在して、徐々に分散され、溶融されていく。最終的に混練物は出口１６より系外に押出されていく。尚、混練途中に設けたベント口３と４を真空ポンプ２４で吸引して、混練物中の空気等のガスを抜くことで混和性がよくなり分散が向上し、並びにトナー中の残存モノマー成分、残存溶剤成分などを取り除くことができ、不純物除去、臭気低減等をすることができる。
【００２１】
本発明においては、連続式押出機の溶融部に供給する方がトナー微粉の分子切断が少なくて好ましい。トナー微粉を押出機の入口付近の粉体部（または固体部）に供給した場合にはニーディングゾーンでの分子切断が大きくなり好ましくない。従って、トナー微粉は混練機中で混練物が固体状態から溶融状態に変化する最初のニーディングゾーンより後に位置する溶融層部にトナー微粉を供給するのが更に好ましい。また、トナー微粉は予め樹脂等と予備混合した後に混練工程の途中に供給してもよい。連続式押出機の軸数としては１軸または２軸がよい。混練機のスクリュタイプは２条、３条または４条などから分散性、生産性、混練温度等を考慮して適宜選択し、スクリュ構成も各種あるスクリュを組み合わせて使用すればよい。
【００２２】
混練機へのトナー微粉の供給は頂部位置に設けたベント口よりスクリューフィーダー等で自然落下または強制供給するか、或いはサイド位置に設けたサイド口よりスクリューフィーダー等で強制供給してもよいが、供給口での閉塞しにくい面から頂部のベント口から供給するのが好ましい。更に、供給口でのトナー微粉の閉塞を防止する為に供給口周辺を水冷等で冷却して、トナー微粉の溶融温度以下に制御する方がより好ましい。
【００２３】
【発明の効果】
本発明の静電荷像現像用トナーの製造方法を用いることにより、多量のトナー微粉でも生産性よく製造工程にリサイクルすることができ、微粉リサイクルしたトナーの性能劣化が少なく、定着性能が良好で、連続使用時でも画像・画質特性が安定しており、耐久性能の優れたトナー性能を与えるなど多大な工業的利益を提供するものである。
【００２４】
【実施例】
下記実施例中、単に「部」とあるのはいずれも「重量部」を意味するものとする。
【表１】

Figure 0003591010
【００２５】
の主原料を配合し、ナウターミキサーで混合し、連続式押出機（（株）池貝製
ＰＣＭ−４６）で混練し、冷却し、粗粉砕後にジェットミル粉砕、風力分級して平均粒径９μｍの黒色トナーを得た。この黒色トナー１００重量部に対してシリカ粉末（日本アエロジル（株）Ｒ９７２）０．３５部とマグネタイト微粉末（戸田工業（株）ＥＰＴ１０００）０．２部をヘンシェルミキサーにて外添処理し、外添トナーを得た。このトナー４部とメチルシリコーン含有樹脂で表面コートされたＣｕ−Ｚｎ−フェライトキャリア（平均粒径＝１００μｍ）９６部をＶ型混合機で攪拌・混合し現像剤を作製した。
【００２６】
本現像剤をスタート用現像剤とし、外添トナーを補給トナーとして、負荷電性有機光半導体の感光体を装着した複写速度６０枚／分の複写機にて３０，０００枚の実写テストを実施した。さらに、複写速度６０枚／分見合いの通紙速度で定着試験を実施し使用温度域を確認した。
実施例及び比較例の各結果を表１に示す。
【００２７】
＜実施例１＞連続押出機（株）池貝製ＰＣＭ−４６の概略図を図３〜５に示し、混練条件は次の通りとした。
【表２】
・混練機のＬ（長さ）／Ｄ（内径）＝３５
・スクリュ軸数：２軸（同方向回転）
・スクリュ条数：２条
・主原料供給量：３３ｋｇ／Ｈｒ
（主原料供給口１よりスクリュフィーダーを使用し自然落下で供給した）
・トナー微粉供給量：１７ｋｇ／Ｈｒ〔微粉割合は３４％〕
（ベント口２よりスクリュフィーダーを使用し自然落下で供給した）
・ベント真空吸引：ベント口３と４を真空ポンプで吸引した。
【００２８】
実施例１の条件で作製したトナーは定着特性が良好で、実写特性も良好であった。
＜実施例２＞
【表３】
・主原料供給量：３７．５ｋｇ／Ｈｒ
・トナー微粉供給量：１２．５ｋｇ／Ｈｒ〔微粉割合は２５％〕
【００２９】
とした以外は実施例１と同様の混練条件とした。
実施例２で作製したトナーは定着特性が良好で、実写特性も良好であった。
＜比較例１＞
【表４】
Figure 0003591010
【００３０】
を主原料とした以外は実施例１と同様の混練条件としたが、主原料の混練機への食い込み状態がやや悪く、原料供給量を５０ｋｇ／Ｈｒから４５ｋｇ／Ｈｒに変更して製造した。
比較例１で作製したトナーは定着特性のホットオフセット発生温度が低く、実写テストでのトナー飛散量も多めであり、問題があった。
＜比較例２＞
【表５】
Figure 0003591010
【００３１】
の主原料とした以外は比較例１と同様の混練条件としたが、混練機の主原料供給口で主原料の食い込みが悪く、供給量を４５ｋｇ／Ｈｒから３８ｋｇ／Ｈｒに変更して製造した。
比較例２で作製したトナーは定着特性のホットオフセット発生温度が低く、実写テストでのトナー飛散量も顕著に多く、問題あった。
【００３２】
【表６】
Figure 0003591010

【図面の簡単な説明】
【図１】通常のトナー製造フローの一例
【図２】本発明のトナー製造フローの一例
【図３】連続式押出機の概略図
【図４】図３のＡ−Ａ′断面図
【図５】ニーディング部スクリュー（３１）と送り部スクリュ（３０）の一例
【符号の説明】
１ 主原料供給口１
２ ベント口２
３ ベント口３
４ ベント口４
５ バレル
６ バレルＣ１
７ バレルＣ２
８ バレルＣ３
９ バレルＣ４
１０ バレルＣ５
１１ バレルＣ６
１２ バレルＣ７
１３ バレルＣ８
１４ バレルＣ９
１５ ダイ
１６ 出口
２０ 主原料ホッパー
２１ スクリュフィーダー
２２ トナー微粉ホッパー
２３ スクリュフィーダー
２４ 真空ポンプ
３０ 送り部スクリュ
３１ ニーディング部スクリュ[0001]
[Industrial applications]
The present invention relates to a method for producing an electrostatic image developing toner used in electrophotography, electrostatic recording, and the like.
[0002]
[Prior art]
In a developing process, a developer used in an electronic copying machine or the like is once attached to an image carrier such as a photoconductor on which an electrostatic image is formed, and then transferred from the photoconductor to transfer paper in a transfer process. Then, in a fixing step, the sheet is fixed on the copy paper surface. At this time, as a developer for developing an electrostatic charge image formed on the latent image holding surface, a two-component developer composed of a carrier and a toner and a one-component developer that does not require a carrier (magnetic toner, non-magnetic toner )It has been known.
As the toner contained in the developer, there are a positively charged toner and a negatively charged toner. Conventionally, those which impart a chargeability to the positively charged toner include nigrosine dyes, quaternary ammonium salts and the like. Further, as a charge imparting agent for imparting chargeability to the negatively charged toner, a charge control agent such as a gold-containing dye or a coating agent imparting a predetermined chargeability to a carrier has been known.
[0003]
FIG. 1 shows an example of a toner production flow that is usually performed. First, a predetermined amount of a resin and a material such as a colorant are mixed and mixed, melt-kneaded in a kneader, cooled, pulverized, and classified. Further, after the classified toner and the external additive are stirred and mixed, a coarse substance is sieved and filled into a container.
Conventionally, as described in Japanese Patent Application Laid-Open No. 5-34976, a predetermined amount of the generated toner fine powder is recycled to a raw material blending / mixing process in consideration of the environment and production cost, and is reused. I was However, according to the conventional toner fine powder recycling method, when the toner fine powder is melted and kneaded again by the kneading machine, the resin molecules in the toner fine powder are cut again, and the fixing performance such as toner hot offset due to a decrease in the molecular weight of the resin is deteriorated. However, this is not preferable because durability performance is deteriorated due to a decrease in mechanical strength. In particular, a decrease in the molecular weight of the resin in the toner tends to occur remarkably when a resin containing a crosslinking component or a resin having at least two molecular weight peaks composed of a low molecular weight compound and a high molecular weight compound is used. Further, when the toner fine powder is mixed with the raw material, (a) the raw material is less likely to be uniformly mixed and the toner composition becomes non-uniform, and (b) the bulk density of the raw material is reduced as compared with the raw material containing no fine powder. When the raw material is supplied to the kneading machine, the biting becomes worse, the toner productivity is lowered, the share at the time of kneading becomes hard to be applied, and the dispersibility of the additive becomes poor. (C) After mixing the raw materials, During the continuous supply from the storage / supply container to the kneading machine, the toner composition becomes uneven during the production process due to the difference in particle size and specific gravity between the raw material and the fine powder inside the storage / supply container. Was apt to be caused, which was not preferable.
[0004]
Particularly, in recent years, the flow softening temperature of the binder resin used for the toner is designed to be lower than that of the fixing surface due to the increase in speed of a copying machine or the like and the reduction of the first copy time. (B) If the toner particle size is reduced due to the high quality of the copy, etc., the classification efficiency is reduced and the fine powder is increased more than before. As a result, the amount of toner fine powder recycled increases, and it has become difficult to secure productivity without deteriorating toner performance.
[0005]
[Problems to be solved by the invention]
Accordingly, a first object of the present invention is to provide a method for producing a toner having a small change in the molecular weight of the toner, and excellent in fixing performance and durability. A second object of the present invention is to provide a method for producing a toner having a uniform composition with good dispersibility of additives in the toner. A third object is to provide a toner which is less dependent on the environment and has excellent storage stability. A fourth object is to provide a toner having stable image characteristics, image quality, charging characteristics, and the like and excellent durability performance even when continuous copying is performed. A fifth object of the present invention is to provide a method for producing a toner having good productivity even when fine powder is recycled.
[0006]
[Means for Solving the Problems]
As a result of various studies by the present inventors, the present inventors have found that toner performance can be improved by recycling and reusing toner fine powder during the kneading step, and arrived at the present invention. That is, the gist of the present invention is to at least mix and mix a resin and a colorant, knead the mixture, then pulverize and classify, and return the generated toner fine powder to the kneading process to reuse the toner to obtain a toner image. In the method for producing a developing toner, an apparatus used in a kneading step is a continuous extruder having at least two kneading zones including kneading screws, and a main material supply port of the continuous extruder for supplying toner fine powder. Located in the direction of the die from
And supplying the toner between the first kneading zone and the second kneading zone .
[0007]
[Action]
Hereinafter, the present invention will be described in detail.
As the resin used in the present invention, known resins suitable for toner can be used. For example, polystyrene, polychlorostyrene, poly-α-methylstyrene, styrene-chlorostyrene copolymer, styrene-propylene copolymer, styrene-butadiene copolymer, styrene-vinyl chloride copolymer, styrene-vinyl acetate copolymer Polymer, styrene-ethyl acrylate copolymer (styrene-methyl acrylate copolymer, styrene-ethyl acrylate copolymer, styrene-butyl acrylate copolymer, styrene-octyl acrylate copolymer and styrene- Phenyl acrylate copolymer), styrene-methacrylate copolymer (styrene-methyl methacrylate copolymer, styrene-ethyl methacrylate copolymer, styrene-butyl methacrylate copolymer, and styrene-phenyl methacrylate) Copolymers), styrene-α-chloro Styrene-based resins such as methyl acrylate copolymer and styrene-acrylonitrile-acrylate copolymer (homopolymer or copolymer containing styrene or styrene substituent), vinyl chloride resin, rosin-modified maleic resin, phenol There are resins, epoxy resins, polyester resins, polyethylene resins, polypropylene resins, ionomer resins, polyurethane resins, silicone resins, ketone resins, ethylene-ethyl acrylate copolymer resins, xylene resins, polyvinyl butyral resins, and polycarbonate resins. Particularly preferred resins for use in the invention include styrene resins, saturated or unsaturated polyester resins, and epoxy resins. In addition, the above resins are not limited to being used alone, and may be used in combination of two or more kinds.
[0008]
The flow softening temperature (Tm) of the resin is preferably from 80 to 150C, more preferably from 90 to 140C. If the temperature is lower than 80 ° C., the fixing temperature to the paper is low and good, but hot offset is apt to occur, and the toner is easily crushed in the developing tank, causing a spent phenomenon in which the toner adheres to the carrier surface and the doctor blade. In addition, there is a problem that the charging characteristics are deteriorated and the durability of the developer is deteriorated. On the other hand, if the temperature is higher than 150 ° C., there are problems such as a high fixing temperature to paper and poor toner crushability.
[0009]
The glass transition temperature of the resin is preferably 45 ° C. or higher. If the temperature is lower than 45 ° C., if the toner is left at a high temperature of 40 ° C. for a long time, the storage stability is poor such that the toner is hardly aggregated or fixed. There are problems in use, such as easy formation of toner aggregates, and adhesion to screens, side walls, and the like of a sieving apparatus to easily form aggregates.
[0010]
In addition, the production of the resin may be performed by known solution polymerization, suspension polymerization, bulk polymerization, emulsion polymerization, or the like, and the polymerization method of each resin component (for example, a low molecular weight substance, a high molecular weight substance, or the like) may be different if necessary. Is also good. Further, the total amount of light-boiling components such as residual monomer and residual solvent in the resin is preferably 2,000 ppm or less, and particularly preferably 1,000 pm or less from the viewpoint of toner odor.
Each test method of the resin used in the present specification will be described below.
[0011]
[Flow softening temperature (Tm)]
In a flow tester (CFT-500 manufactured by Shimadzu Corporation), 1 g of a sample was measured under the conditions of a nozzle of 1 mm × 10 mm, a load of 30 kg, a preheating time of 50 ° C. for 5 minutes, and a heating rate of 3 ° C./min. Then, the temperature at the midpoint of the distance from the start to the end of the flow is defined as the softening temperature.
[0012]
[Glass transition temperature (Tg)]
In a differential thermal analyzer (DTA-40, manufactured by Shimadzu Corporation), a tangent line was drawn at the transition (inflection) start point of the curve measured at a heating rate of 10 ° C./min, and the temperature at the intersection was determined by the glass transition. Temperature.
Known pigments and dyes may be used as the colorant used in the present invention. For example, carbon black, titanium oxide, zinc white, alumina white, calcium carbonate, ultramarine, navy blue, phthalocyanine blue, phthalocyanine green, Hansa yellow G, rhodamine dye, chrome yellow, quinacridone, benzine yellow, rose bengal, triallylmethane Coloring agents such as dyes, anthraquinone dyes, monoazo and diazo dyes and pigments can be used alone or in combination of two or more. The content of the colorant may be an amount sufficient to color the toner so that a visible image can be formed by development, and is, for example, 1 to 20 parts by weight, preferably 3 to 15 parts by weight based on 100 parts by weight of the resin. It is contained by weight.
[0013]
Further, a known positively or negatively chargeable charge control agent may be used alone or in combination in the toner, and the amount of the charge control agent may be selected depending on the desired charge amount. On the other hand, the amount is preferably about 0.05 to 10 parts by weight. Examples of the positive charge control agent include a nigrosine dye, a quaternary ammonium salt compound, a triphenylmethane compound, an imidazole compound, and a polyamine resin. Examples of the negative charge control agent include metal-containing azo dyes such as Cr, Co, Al, and Fe, metal salicylate compounds, metal alkylsalicylate compounds, and curlic arene compounds.
[0014]
Further, if necessary, other internal additives may be used alone or in combination as an auxiliary agent, and examples thereof include known low-molecular-weight olefin polymers and fillers of release agents.
First, an example of the toner manufacturing flow of the present invention will be described with reference to FIG. 2, but the present invention is not limited to the following description unless it exceeds the gist.
Predetermined amounts of at least a resin and a colorant are weighed and blended as the toner internal additive, and they are mixed. Examples of the mixing device include a double cone mixer, a V-type mixer, a drum type mixer, a super mixer, a Henschel mixer, a Nauta mixer and the like.
[0015]
Next, in the kneading step, a batch-type (for example, a pressure kneader, a Banbury mixer, etc.) or a continuous-type kneader is used, but in recent years, a single-screw or twin-screw extruder has been used because of its superiority such as continuous production. The mainstream is, for example, a KTK type twin screw extruder manufactured by Kobe Steel, a TEM twin screw extruder manufactured by Toshiba Machine Co., Ltd., a twin screw extruder manufactured by KCS, and a PCM type twin screw extruder manufactured by Ikegai Iron Works. Machine, a twin-screw extruder manufactured by Kuriyama Seisakusho, a co-kneader manufactured by Bus, and the like are preferable.
After kneading, the toner is rolled by two rolls or the like, and goes through a cooling step of cooling by air cooling, water cooling or the like.
Next, in the pulverizing step, coarse pulverization is performed by a crusher, a hammer mill, a feather mill, or the like, finely pulverized by a jet mill, a high-speed rotor rotary mill, or the like, and pulverized to a predetermined toner particle size in a stepwise manner.
[0016]
After pulverization, the toner is classified using an inertial classification elbow jet, a centrifugal classification microplex, a DS separator, or the like, to obtain a toner having an average particle diameter of 3 to 15 μm. The coarse toner powder generated in the classification step may be returned to the pulverization step and reused.
Further, when externally adding to the toner, a predetermined amount of the classified toner and various known external additives are blended, and the mixture is stirred and mixed by a high-speed stirrer such as a Henschel mixer or a super mixer that applies a shearing force to the powder. Is good. At this time, since heat is generated inside the external additive device and aggregates are easily generated, it is preferable to adjust the temperature by means such as cooling the periphery of the container portion of the external additive device with water. The temperature of the material inside the container is preferably not higher than the control temperature which is about 10 ° C. lower than the glass transition temperature of the resin.
[0017]
As the external additive, various known inorganic or organic external additives can be used. In particular, in order to improve the fluidity of the toner and suppress aggregation, titania, silica, alumina, zinc oxide, magnesium oxide, etc. Inorganic fine powders are preferred.
The mixing amount of the external additive varies depending on the average particle diameter, particle size distribution, and the like of the external additive and the toner particles to be used, but is preferably an amount that obtains the desired toner fluidity. The amount is preferably from 05 to 10 parts by weight, more preferably from 0.1 to 8 parts by weight. If the amount is less than 0.05 part by weight, there is no fluidity improving effect, and the storage stability at high temperatures is poor. If the amount is more than 10 parts by weight, filming occurs on the photoreceptor due to the partially released external additive. Or it is deposited in the developing tank and causes troubles such as deterioration of the charging function of the developer, which is not preferable.
[0018]
In addition, from the viewpoint of stability in a high humidity environment, in the case of an inorganic fine powder, the external additive is more preferably subjected to a hydrophobic treatment with a known treating agent such as silane coupling, and further, in consideration of chargeability. In this case, as a treating agent for imparting negative charge, dimethyldichlorosilane, monooctyltrichlorosilane, hexamethyldisilazane, silicone oil, etc., and an aminosilane as a treating agent for imparting positive charge may be used.
In addition, known magnetites, farites, conductive titanium, antimony oxide, tin oxide, cerium oxide, hydrotalcite compounds, acrylics other than those used for improving fluidity, for the purpose of adjusting the resistance, polishing and the like as toner external additives. Fine powders such as beads, silicone beads, polyethylene beads and the like may be appropriately mixed, and the mixing amount is preferably 0.005 to 10 parts by weight based on 100 parts by weight of the toner.
[0019]
The obtained toner is a one-component developer not using a carrier (a magnetic one-component toner containing a magnetic substance such as magnetite or a non-magnetic one-component toner containing no magnetic substance), or an iron powder, ferrite, or magnetite. And a two-component developer mixed with a magnetic carrier such as a magnetic resin carrier.
FIG. 2 shows an example of the toner production method of the present invention. The present invention is characterized in that the toner fine powder is supplied during the kneading step, and is particularly effective when the toner fine powder is supplied during the continuous extruder. Act on.
[0020]
FIG. 3 shows an example of a continuous extruder.
The barrel is divided into 10 sections of 5 to 14, and 9 barrels of barrels 6 to 14 and the die 15 have an electric heater inside or outside, and the temperature is controlled by a temperature control panel. The barrel 5 has a main material supply port 1 at an upper portion, and has vent ports 2, 3, and 4 at upper portions of the barrel 9, the barrel 11, and the barrel 13, respectively. Inside the extruder, there is provided a screw that engages two double-type shafts and rotates at a high speed of about 100 to 500 rpm in the same direction. The configuration of the screw can be appropriately selected. For example, as shown in FIG. 3, the screw may be configured to include a feed screw 30 and a kneading screw 31. The main toner raw material is supplied from the main raw material hopper 20 to the main raw material supply port 1 by the screw feeder 21 and supplied to the feed screw 30. The main raw material is gradually preheated, and when the first kneading portion screw 31 has a strong share, the raw material is dispersed by self-heating of the main raw material itself, and changes from a solid state to a molten state. At the time of passing through the barrel 9, the main raw material is in a sufficiently molten state. Here, the toner fine powder is injected into the vent port 2 from the hopper 22 by the screw feeder 23, and the toner fine powder and the molten main raw material are combined. In the subsequent feed screw and kneading screw, the toner fine powder is mixed with the main raw material, and is gradually dispersed and melted. Finally, the kneaded material is extruded from the outlet 16 to the outside of the system. The vent ports 3 and 4 provided during kneading are sucked by a vacuum pump 24 to remove gas such as air from the kneaded material, whereby the miscibility is improved, the dispersion is improved, and the residual monomer component in the toner is improved. In addition, residual solvent components can be removed, and impurities can be removed and odor can be reduced.
[0021]
In the present invention, it is preferable to supply the toner to the melting part of the continuous extruder because the molecular cutting of the toner fine powder is small. When the toner fine powder is supplied to the powder portion (or solid portion) near the entrance of the extruder, the molecular cutting in the kneading zone becomes large, which is not preferable. Therefore, the toner fines kneaded mixture is further preferred to feed the toner fines to the molten layer section located after the first kneading zone change into a molten state from a solid state in a kneader arbitrariness. Further , the toner fine powder may be supplied in the middle of the kneading step after being preliminarily mixed with a resin or the like. The number of axes of the continuous extruder is preferably one or two. The screw type of the kneading machine may be appropriately selected from two, three or four in consideration of dispersibility, productivity, kneading temperature and the like, and various types of screws may be used in combination.
[0022]
The supply of the toner fine powder to the kneader may be naturally dropped or forcibly supplied by a screw feeder or the like from a vent port provided at a top position, or may be forcibly supplied by a screw feeder or the like from a side port provided at a side position. It is preferable to supply from the vent port at the top from the surface which is hard to block at the supply port. Further, it is more preferable to cool the periphery of the supply port with water cooling or the like to prevent the toner fine powder from being blocked at the supply port, and to control the temperature to be equal to or lower than the melting temperature of the toner fine powder.
[0023]
【The invention's effect】
By using the method of manufacturing a toner for developing an electrostatic image of the present invention, even a large amount of toner fine powder can be recycled to the manufacturing process with high productivity, and the performance of the fine powder recycled toner is small, and the fixing performance is good. Even when used continuously, the image and image quality characteristics are stable, and a great industrial advantage is provided, such as giving a toner having excellent durability.
[0024]
【Example】
In the following examples, “parts” simply means “parts by weight”.
[Table 1]
Figure 0003591010
[0025]
Are mixed with a Nauter mixer, kneaded with a continuous extruder (PCM-46 manufactured by Ikegai Co., Ltd.), cooled, coarsely pulverized, then jet mill-pulverized, and air-classified to have an average particle diameter of 9 μm. Was obtained. To 100 parts by weight of this black toner, 0.35 parts of silica powder (R972 by Nippon Aerosil Co., Ltd.) and 0.2 parts of magnetite fine powder (EPT1000 by Toda Kogyo Co., Ltd.) were externally added using a Henschel mixer. An additional toner was obtained. 4 parts of this toner and 96 parts of a Cu—Zn-ferrite carrier (average particle size = 100 μm) surface-coated with a methyl silicone-containing resin were stirred and mixed with a V-type mixer to prepare a developer.
[0026]
Using this developer as a starting developer and using externally added toner as replenishing toner, a 30,000-sheet copying test was performed on a copying machine equipped with a photoconductor of a negatively chargeable organic optical semiconductor at a copying speed of 60 sheets / min. did. Further, a fixing test was carried out at a paper passing speed corresponding to a copying speed of 60 sheets / min to confirm a use temperature range.
Table 1 shows the results of Examples and Comparative Examples.
[0027]
<Example 1> Figs. 3 to 5 are schematic diagrams of PCM-46 manufactured by Ikegai Continuous Extruder Co., Ltd., and the kneading conditions were as follows.
[Table 2]
・ L (length) / D (inner diameter) of kneader = 35
・ Number of screw shafts: 2 (rotation in the same direction)
・ Number of screw strips: 2 ・ Main raw material supply: 33 kg / Hr
( Supplied naturally from the main material supply port 1 using a screw feeder)
-Supply amount of toner fine powder: 17 kg / Hr [fine powder ratio is 34%]
(Supplied naturally from the vent 2 using a screw feeder)
Vent vacuum suction: The vent ports 3 and 4 were suctioned by a vacuum pump.
[0028]
The toner produced under the conditions of Example 1 had good fixing characteristics and good actual photographing characteristics.
<Example 2>
[Table 3]
・ Main raw material supply: 37.5 kg / Hr
-Supply amount of toner fine powder: 12.5 kg / Hr [fine powder ratio is 25%]
[0029]
The kneading conditions were the same as in Example 1 except for the above.
The toner produced in Example 2 had good fixing characteristics and good actual photographing characteristics.
<Comparative Example 1>
[Table 4]
Figure 0003591010
[0030]
The kneading conditions were the same as in Example 1 except that was used as the main raw material, but the state of biting of the main raw material into the kneader was slightly poor, and the raw material supply was changed from 50 kg / Hr to 45 kg / Hr.
The toner manufactured in Comparative Example 1 had a problem that the hot offset generation temperature of the fixing property was low and the amount of toner scattered in the actual photographing test was large.
<Comparative Example 2>
[Table 5]
Figure 0003591010
[0031]
The kneading conditions were the same as in Comparative Example 1, except that the main raw material was not used, but the main raw material was not well penetrated at the main raw material supply port of the kneader, and the supply amount was changed from 45 kg / Hr to 38 kg / Hr. .
The toner produced in Comparative Example 2 had a problem that the hot offset generation temperature of the fixing property was low and the amount of toner scattered in the actual photographing test was remarkably large.
[0032]
[Table 6]
Figure 0003591010

[Brief description of the drawings]
FIG. 1 is an example of a normal toner production flow. FIG. 2 is an example of a toner production flow of the present invention. FIG. 3 is a schematic diagram of a continuous extruder. FIG. 4 is a sectional view taken along line AA ′ of FIG. An example of the kneading screw (31) and the feed screw (30)
1 main raw material supply port 1
2 vent port 2
3 vent port 3
4 vent ports 4
5 barrels 6 barrels C1
7 barrel C2
8 barrel C3
9 barrel C4
10 barrel C5
11 barrel C6
12 barrel C7
13 barrel C8
14 barrel C9
15 Die 16 Outlet 20 Main material hopper 21 Screw feeder 22 Toner fine powder hopper 23 Screw feeder 24 Vacuum pump 30 Feed screw 31 Kneading screw

Claims (4)

少なくとも樹脂及び着色剤を配合、混合した後、混練し、次いで粉砕、分級するとともに、発生したトナー微粉を混練工程に戻して再利用してトナーを得る静電荷像現像用トナーの製造方法において、混練工程で使用される装置がニーディング部スクリュからなるニーディングゾーンを少なくとも２つ有する連続式押出機であり、トナー微粉を該連続式押出機の主原料供給口からダイの方向に位置する第１のニーディングゾーンと第２のニーディングゾーンとの間に供給することを特徴とする静電荷像現像用トナーの製造方法。At least a resin and a colorant are blended and mixed, then kneaded, then pulverized and classified, and the method for producing a toner for developing an electrostatic image is obtained in which the generated toner fine powder is returned to the kneading step and reused to obtain a toner. The apparatus used in the kneading step is a continuous extruder having at least two kneading zones consisting of a kneading part screw, and the toner fine powder is positioned in the direction of the die from the main material supply port of the continuous extruder. A method for producing a toner for developing electrostatic images, wherein the toner is supplied between a first kneading zone and a second kneading zone. 第１のニーディングゾーンと第２のニーディングゾーンとの間の位置を真空ポンプで吸引することを特徴とする請求項１に記載の静電荷像現像用トナーの製造方法。The method of producing an electrostatic charge image developing toner according to claim 1, characterized in that for sucking position between the first kneading zone and a second kneading zone with a vacuum pump. ダイとダイから最も近いニーディングゾーンとの間の位置を真空ポンプで吸引することを特徴とする請求項１または２に記載の静電荷像現像用トナーの製造方法。The method according to claim 1 , wherein a position between the die and a kneading zone closest to the die is suctioned by a vacuum pump. 連続式押出機のスクリュー軸数が１軸又は２軸であることを特徴とする請求項１乃至３の何れかに記載の静電荷像現像用トナーの製造方法。4. The method according to claim 1, wherein the number of screw axes of the continuous extruder is one or two.
JP26913194A 1994-07-29 1994-11-01 Method for producing toner for developing electrostatic images Expired - Fee Related JP3591010B2 (en)

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US5846683A (en) * 1996-04-08 1998-12-08 Sharp Kabushiki Kaisha Toner producing method using recycled extra-fine toner particles
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JPH1130876A (en) * 1997-05-12 1999-02-02 Ricoh Co Ltd Full-color electrophotographic toner, method for producing the same and image forming method
US6326119B1 (en) * 2000-03-07 2001-12-04 Xerox Corporation Toner and developer providing offset lithography print quality
JP4850006B2 (en) * 2006-09-13 2012-01-11 株式会社リコー Toner for electrophotography and method for producing toner
CH706511A1 (en) * 2012-05-15 2013-11-15 Bba Innova Ag A process for producing powder of a more granular, thermoplastic material and apparatus for producing chips from a powdered thermoplastic material.
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US5272034A (en) * 1991-07-22 1993-12-21 Mita Industrial Co., Ltd. Process for producing electrophotographic toner
US5376494A (en) * 1991-12-30 1994-12-27 Xerox Corporation Reactive melt mixing process for preparing cross-linked toner resin
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